関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Phosphoric Acid | HCID 1004 | — |
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | HCID 23675546 | HCID 23675546 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | Trifop-methyl | HCID 94586 | — |
反応手順
63 g of dimethyl sulfate are added within 5 minutes and at 130° C. to 348 g of anhydrous sodium-2-[4'-(4"-trifluoromethyl-phenoxy)-phenoxy]-propionate, suspended in 1,000 ml of xylene. After the addition, stirring of the mixture is continued for 1 hour, the mixture is cooled at 85° C., at said temperature 200 ml of water and 0.5 ml of H3PO4 are added and, for the separation of the inorganic salts, the mixture is stirred for 10 minutes. After separation of the water phase, the xylene is distilled off. 340 g of methyl-2-[4'-(4"-trifluoromethyl-phenoxy)-phenoxy]-propionate are obtained melting at 142° C. under 0.05 torr. According to gas chromatogram the content of pure final product is 99.4%, the residual content of unreacted acid is 0.6%, which corresponds to a yield of 99.4%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04252980 |
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| 出典データセット | uspto-grants-1981_02 |
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| ORD ID | ord-4c4ffb351c7643d1bc21a5c46786903b |
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| 出典メモ | uspto-grants-1981_02 |
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